Process and device for fractional distillation of liquid mixtures, more particularlypetroleum



Sept. 8, 1942. BRUGMA 2,295,256 -PROCESS AND DEVICE FOR FRACTIONAL DISTILLATION OF LIQUID MIXTURES,

- MORE PARTICULARLY PETROLEUM Original Filed Dec. 1, 1936 4 Sheets-Sheet 1 INVENTOR= ANTOI JOHA BRUG-MA ATTORNEY Sept. 8, 1942.

A. J. BRUGMA 2,295,256 PROCESS AND DEVICE FOR FRACTIONAL DISTI LLATION OF LIQUID MIXTURES, MORE PARTICULARLY PETROLEUM Original Filed Dec. 1, 1936 4 Sheets-Sheet 2 Sept. 8, 1942, J; BRUGMA 2,295,256

PRocEss AND DEVICE FOR FRACTIONAL DISTILLATION OF LIQUID MIXTURES MORE PARTICULARLY PETROLEUM Original Filed Dec. 1, 1936 4 Sheets-Sheet 3 VENTOR= IN ANTOINE JOHAN B GMA BM- ATTORNEY Sept. 8, 1942. J BRUGMA 2,295,256

PROCESS AND DEVICE FOR' FRACTIONAL DISTILLATION OF LIQUID MIXTURES,

MORE PARTICULARLY PETROLEUM Original Filed Dec. 1, 1936 4 Sheets-Sheet 4 INVENTOR=.

ANTOINE JOHAN BUGMA ATTORNEY Patented Sept. 8, 1942 PROCESS AND DEVICE FOR FRACTIONAL DISTILLATION OF LIQUID MIXTURES, MORE PARTICULARLY PETROLEUM Antoine Johan Drum, The Hague, Netherlands Continuation of application Serial No. 113,596, December 1, 1936. This application August 23, 1940, Serial No. 353,788. In the Netherlands January 30, 1936 6 Claims. (Cl. 196-73) This invention relates to the fractional distillation of composite fluids such as hydrocarbon oils and the like. 1

This application is a continuation of application Serial No, 113,596, filed December 1, 1936.

The invention provides a novel method and novel apparatus for accurately separating the components of a composite fluidwithout the necessity of utilizing stripping of intermediate fractions. For example, the practice of the invention makes it possible to obtain four closely fractionated products from a feed stream by using two towers only with no side stream strippers, and to obtain eight closely fractionated products by using three towers only with no side stream strippers. Use of the invention results in a saving in ground space and in first cost of the equipment.

In carrying out the invention, a single feed stream is introduced into a first fractionatin tower wherein the feed is substantially complete-- 1y fractionated into two non-overlapping fractions, after which these two fractions are introduced into a second fractionating tower at spaced points, and two substantially non-overlapping fractions are removed from the second tower at points intermediate the points 'at which the two fractions from the first tower are introduced into the second tower in addition to the overhead and bottoms streams from the second tower. If desired, the two overlapping fractions removed from the second tower may be introduced into a third tower together with the overhead and bottom streams from the second tower. From the third tower, two well fractionated streams are removed intermediate the points of introduction of each pair of feed streams to the third tower, in addition to the overhead and bottom streams from the third tower. I

It is well known that in the operation of a fractionating or rectifying column, each tray above the point of feed will contain liquid which is richer in light constituents of the feed material and is poorer in heavy constituents than the liquid on the tray or trays at a lower elevation. In consequence, it has been possible to obtain one or more fractions of intermediate composition from the column'by withdrawing liquid from one ,or more of the trays ef the column. This method however, is disadvantageous because the intermediate fractions thus obtained will contain as impurities all the constituents from the top fraction if the tray or trays from which liquid is withdrawn are located above the feed point to the column, whereas'these intermediate fractions 5 will contain constituents of the bottom fraction if the tray or trays from which the liquid is withdrawn are located below the feed Point. This is through the liquid on the trays above the point of feed so that on each of these trays the vapor and liquid will be'in approximate equilibrium and the constituents of the top fraction will be present in the liquid in a certain ratio. This is also true of the liquid withdrawn from the trays disposed below the point of feed so far as the constituents of the bottom fraction are concerned. It is not possible therefore, to obtain intermediate fractions from fractionating columnsutilized heretofore which do not overlap each. other at all or only to a, very slight degree with regard to the boiling points of their constituents, which means that redistilling will often be needed which will necessitate extra apparatus, fuel, tank space and labor.

These disadvantages of prior fractionating methods are overcome by the present invention. Fractions withdrawn from the trays of fractionating columns arranged and operated in accordance with the invention will not overlap each other at all; or will only overlap each other to a very slight degree.

The invention will be understood from the following description considered in connection with the accompanying drawings forming a part thereof, and in which: i

Fig. l is a diagrammatic view showing fractionating apparatus illustrating a conventional distillation method Fig. 2 Isa-view similar to Fig. 1, but showing a form ofapparatus illustrating the principles of the invention},

Fig/3 isa diagrammatic view illustrating one form of. apparatus embodying and operated in accordance with the invention, and

Fig. 4 is a diagrammatic view showing another form of apparatus embodying and operated in accordance with the invention.

Like characters of reference refer to the same or to similar'parts throughout the several views.

Referring to the drawings, particularly Figs. 1 and 2, reference character I designates a single fractionating column or tower into which com-. posite fluid, such as hydrocarbon oil or the like, is introduced onto one of the intermedite trays of the column, the fluid so introduced or the feed, containing for example fractions A, B, C L and D. Within the column I, the feed will be completely separated into a top fraction A+B and a bottom .fraction C+D provided the tower is operating in an ideal manner, so that the top and bottom fractions will not overlap each other. These two fractions, A+B and C'+D, are then introduced into two other fractionating columns or towers 2 and 3, with the result that each of these fractions is completely separated into two one above the other and to heat the still of the upper column 2, by means of the condenser of the lower column 3, so that the amount of heat applied to the column 3 will serve: for both columns with the result that both columns will consume I about one-half of the amount of heat and cooling water needed for the fractionating apparatus shown in Fig. 1. Such an arrangement is illustrated in Fig. 2, which shows the same fractionating apparatus as shown in Fig. 1, with the exception that a two coil circulating system 50 is provided in which a heat transferring fluid is circulated by a pump 5|. One of the coils is disposed in the condenser of the lower column 3, and the other coilis located in the still of the upper column 2, so that the still is heated by heat transferred from the condenser of the lower column 3. In the same manner, the four columns which receive the four fractions A, B, C and D,

r I and reflux is returned to the top of the tower the condenser of column 3 and the still of column 2, and connecting these columns by means of a similar column, whereby they are combined into one column. The intermediate portion of this one column will then serve as a heat transmitter in the manner hereinbefore described.

An arrangement of this character is shown diagrammatically in Fig. 3. Referring to that flgure, the fluid mixture which is to be separated into fractions A, B, C, D, E, F, G and H, is introduced through feed line 4 into the fractionating column I of any desired type. Column I is provided at the time with 'a condenser 5 and at the bottom with a still 6. Vapor is conducted from the column to the condenser 5 through line through line 8. Bottoms are conducted from the column to the still 3 through line 9 and vapor is returned to the bottom of the column from the still through line III. In column I the feed liquid is separated in a practically perfect manner into a fraction A+B+C+D which is with- Fractionating column 2 consists essentially of two fractionating columns II and I3 which may be placed'one above the other, so that the amount of heat and cooling water will serve for all four columns. This arrangement may be carried on to the extent of the fractionation desired.

In lieu of supplying to a still the heat'from the condenser for the column disposed below, the still and condenser may be removed and the adjacent superimposed columns may be connected with an intermediate fractionating column thereby obtaininga single column having a height equal to the height of the two original columns and the height of the intermediate or connecting column. The intermediate column will convey the heat unwardly therethrough and at the same time will maintain the difference in composition between the liquids on the trays above and below the intermediate column. In this manner the still and condenser are replaced by the top and the bottom trays of the intermediate or connecting column, from which trays the corresponding fractions are withdrawn from the fractionating column.

Inasmuch as the temperature in the condenser of column 3 of Fig; 1, will be higher than the temperature in the still of column 2 of Fig. 1, it will be possible-to heat the still of column 2 by means of the condenser of column 3, thereby conveying the heat supplied to the-still of column 3 successively through the: columns 3 and 2 and to deliver the heat to the cooled water of the condenser of column 2. Assuming that columns -2 and 3 consume substantially equal amounts of are connected by a heat transmitting column I2. To the upper column I3 is connected line I4 and to the lower column is connected line I3. Column 2 is provided with a condenser It to which vapor is conducted through line II and from which reflux is returned to the top of the column through line I9. Column 2 is also provided with a still I8 to which bottoms are conducted through line 2| and from which vapor is conducted to the bottom of column 2 through line 20. In column 2, the fraction A+B+C+D which is introduced into .the upper portion I3 of the column 2, is

separated in a practically perfect manner into two fractions, consisting respectively of 4+8 and C+D, and the fraction consisting of E+F+G+H which is introduced into the lower portion II of column 2, is separated in a practically perfect manner into two fractions consisting respectively of E+F and G+H. The fraction A-I-B is conducted-to the condenser I6 and is withdrawn therefrom through line 22, and the fraction G-I-H is conducted to still I3 from the bottom of the column and is withdrawn therefrom through line 25. The fraction C+D is withdrawn through line 23 which is connected to the column 2 at a point above the heat transmitting portion I2 of the column, and the fraction E+F is withdrawn from the column through line 24 which is located below the heat transmitting portion I2.

The column 3 consists essentially of four fractionating columns 26, 21, 28 and 20 and three heat transmitting portions 30, 3|, and 32, and is provided with a still 42 and connecting lines 43 and 44, and a condenser 4| with connecting lines stock into a greater number of fractions than eight, another fractionating column similar to column 3, may be utilized with the discharge lines of column 3 connected thereto as feed lines, and having sixteen discharge lines, such other column operating in the same manner as columns 2 and 3. Also if desired, one or more of the fractions withdrawn from columns 2 or 3 may be conducted to a point of use rather than being introducedqnto a succeeding column, or such withdrawn fractions may be separated otherwise individually into two or more fractions. Pumps or control valves or both may be provided in the connecting lines between the several columns.

Obviously the apparatus in which the process is carried out, may be provided with any equipment for promoting good distillation, economical heating and so forth. such for example as heat exchangers, preheaters and so forth, while a pretreating device for the feed stock may be employed in connection with the apparatus, such as a tube still with a vaporizer for separating the residue, or equipment for after treatment or distillation of one or more of the fractions may be utilized. The stills, columns and condensers may be of different arrangements and may be interconnected differently.

It will be understood that the invention may be carried out in two columns, such as in columns I and 2 of Fig. 3, or in more than three columns which are arranged in the manner illustrated in Fig. 3.

Another form of apparatus for carrying out the invention is shown in Fig. 4. This apparatus is the equivalent of columns I and 2 and the associated equipment of Fig. 3, excepting that column 2 is divided into two parts whichare placed side by side. Column II in Fig. 4 is the equivalent of section II of column 2 of Fig. 3, and the column consisting of the sections I2 and I3 in Fig. 4 is the equivalent of sections I2 and I3 of column 2 of Fig. 3. Vapor line 60 connects column II with section I2 in Fig. 4, and a liquid iineSI having a pump 62 therein connects the bottom of section I2 with the upper part of column II. Such an arrangement does not alter the principles of the invention because the fractionating zone and tower are merely divided into two or more parts which function as a single fractionating zone or tower. Hence in the foregoing description and in the claims, where it is stated that fractions are introduced at two successive points into a fractionating tower or zone, it will be understood that either an undivided or a divided fractionating tower or zone is meant. For example in Fig. 4, the fractions A+B+C+D and E+F+G+H are introduced into the fractionating zone at two successive points, since column l2, I3 in Fig. 4 constitutes a continuation of column I I, inasmuch as these two columns II and I2, I3 together form only one fractionatmg zone to which heat is supplied by still I8 and I8. As previously mentioned, the advantages of from which heat is withdrawn in condenser the invention include economy of heat and cooling water due to the utilization of the same quantity of heat and cooling water for a multiple fractionation, and the sharply defined separation in which the fractions obtained do not overlap at all or overlap only to a very slight extent.

It will be understood that changes may be closed, and changes may be made in the sequence,

of the several steps of the process, without departing from the principles of the invention, wherefore the invention is not to be limited excepting by the scope of the appended claims.

What is claimed-is:

L'The method of fractionally distilling fluid mixtures in at least three stages, each stage comprising a fractionating zone in which a stream of vapors is contacted in counter-current with the stream of liquid condensed therefrom while after the first stage, apart from other :fractions, at least twice, two side stream fractions are withdrawn from a fractionating zone at spaced levels intermediate two successive points at which fractions from the preceding stage are introduced.

2. The method of fractionally distilling composite fluids which comprises introducing fluid into a first fractionating zone, substantially completely separating the fluid into a plurality of fractions in said zone, withdrawing a plurality of said fractions from said zone and introducing them at different points into a second fractionating zone, withdrawing a plurality of inter-- mediate fractions from the second fractionating zone between adjacent points at which the flrst mentioned fractions are introduced into the second zone, withdrawing an overhead and a bottoms fraction from the second zone, introducing said overhead and bottoms fractions and a plurality of said intermediate fractions into a third fractionating zone at spaced points thereof, and withdrawing a plurality of intermediate fractions from said third zone between adjacent points at which fractions from the second zone are introduced.

3. The method of fractionally distilling composite fluids which comprises introducing fluid into a first fractionating zone, substantially completely separating the fluid into a plurality of fractions in said zone, withdrawing a plurality of said fractions from said zone and introducing them at diiferent points into a second fractionating zone, withdrawing two intermediate fractions from the second fractionating zone between adjacent points at which the first mentioned fractions are introduced into the second zone, introducing said intermediate fractions into a third fractionating zone at spaced points thereof, and'withdrawing two intermediate fractions from said third zone between adjacent points at which said fractions from the second zone are introduced.

4. Apparatus for the fractional distillation of 5. Apparatus for the fractional distillation'of composite fluids comprising three fractionating towers,'means for introducing fluid into the flrst tower, means for conducting fractions from the first tower to spaced points in the second tower, means for withdrawing two intermediate fractions from the second tower between adjacent points at which fractions from the first tower are introduced, means for withdrawing an overhead and a bottoms fraction from the second tower, means for delivering the overhead and bottoms fraction and said intermediate fractions to spaced points in the third tower, and means for withdrawing two fractions-from the third tower between adjacent points at which fractions are introduced into the third tower.

6. The method of fractionally distilling composite fluids to produce in two fractionating tionating zone to provide a stripping mediumfor said stripping zone, separately conducting the other portion of the overhead stream and the reflux leaving the lower portion of the fractionating zone to a second fractionating zone as flrst and second feed streams respectively, the constituents of said first and second feed streams being substantially completely separated from each other, introducing the flrst feed stream into the second fractionating zone at an intermediate point of its upper part above a stripping zone and below a-rectifying zone therein, introducing the second feed stream into the second fractionating zone at an intermediate point of its lower part above a stripping zone andbelow a rectifying zone therein, the second fractionating zone having a heat transmitting and fractionating zone between the stripping .zone of the upper part vand the rectifying zone of the lower part'which serves to transmit heat from the'lower'to the upper parts of the second fractionating zone, removing an'overhead stream from the second fractionating zone, condensing at least a portion of said last mentioned stream and returning condensate to the upper part of the second fractionating zone as reflux, vaporizing a portion of the reflux leaving the lower part of the second fractionating zone to provide a stripping medium for the stripping zone in the lower part of the second fractions-ting zone, the other portion of the overhead stream constituting a flrst fraction,

withdrawing a second intermediate fraction from the second fractionating zone at the base of the stripping zone of the upper'part thereof, withdrawing a third intermediate fraction from the second fractionating zone at the top of the rectifying zone of the lower part thereof, the other portion of the reflux leaving the lower part of the second fractionating zone constituting a fourth fraction, the constituents of said first, second,' third and fourth fractions being substantially completely separated from each other, and said heat transmitting and fractionating zone serving to maintain the separation between the constituents of the first and second feed streams effected in the first fractionating zone.

ANTOINE JOHAN BRUGMA. 

